Process of distilling solids and liquids and of cracking solids, liquids, and gases



y A. 1. PARIS, JA. PRocEss oF msmunm somos AND uoum's AND oF cRAcmNG somos, Llouws, AND GASES;

APPLICATION FILED MAY 31 I9L5. lggs', Patentedet. 4, 1921.

' i 2 SHEETS-SHEET l.

WITNESS.'

n A. 1. PARISJR. PROCESS 0F DISTILLING SOLIDS ANDKLIQUIDS AND 0F CRACKING SOLIDS, LIQUIDS, AND GASES* APPLICATION FILED MAY 3*, I9I5. LSQJSSI, Patented Oct. 4, 1921L 2 SHEETS-SHEET 2.

vk @J l l I a" I I I @h4 I" I I' Il l UNITED STATES AUGUSTE J. PARIS, JR., or

PATENT OFFICE..

BRADFORD. PENNsYLvAinA CRACKING soLIDs, LIQUIDS,

Application led May 3 To all whom t may concern Be it known that I, AUGUSTE JEAN PARIS, Jr., a citizen of the United States, residing in Bradford, county of McKean, and State of Pennsylvania, have invented a certain new and useful ,Process ofDistilling Solids and Liquids and of4 Cracking Solids, Liquids, and Gases, of which the following is a specification. Y

This invention is a process of distilling solids and liquids andlof cracking solids, liquids and gases, and the objects of the invention, speaking generally, are to distil saidy liquids and solids underv conditions which enable the pressures, either plus or minus, and the temperatures to be accurately and effectively controlled, and to permit of Ithe cracking of the various materials under similar conditions of control.

Heretofore, serious difficulties have existed in connection with the cracking of hydrocarbons, because of the fact, among others, that the separated carbon accumulated and caked at the .bottom of the still, the point at which the heat for distillation is applied, andv eventually resulted in the burning out of the bottoms of the stills or retorts.

Moreover, even in the ordinary processes of distillation, where cracking is not specially aimed at, there is usually some deposit of carbon and always a deposit of other residues, which occasion the same dis- 1 advantages referred to in connection with the cracking processes.

The p resent invention overcomes the disadvantages Ireferred to, -as well as' others, and embodies, as one of its salient features, a still, or other receptacle, wherein the solid, liquid, or gaseous material is treated, in which still is contained a molten mass of metal, preferably lead, through which the materials treated are passed or brought into contact with, depending on the particular operation being performed.

Speaking generally, the advantages of employing a molten bath of metal, for the purposes specified, are as follows: First, the bottom of the still is kept entirely free from any deposit of carbon or other residues, this result being effected, mainly, because of the fact that the agitation of the molten metal, through boiling, keeps the bottom of the still or retort clean; the separated material, such as carbon or residues,

Specification Bf Letters Patent.

Patented oet. a, met.

,19;5. serial No. 25,403.

. being of less specific gravity than the bath,

flows to the surface of the latter, and, in its passage through the metal becomes disintegrated, that is to say, is kept from caking; second, in the cracking or similar operation, there is an intimate and extended contact -of the 4material treated with the molten metal, thereby allowing ample time for the completion of the chemical-reactions desired; third, the temperature can be 'uniformly controlled at the same degree as, or above that, of the molten bath employed,

" and this can be easily effected automatically; this can be accomplished by regulating the quantity of heat applied `to the still, or by keeping the quantity of heat constant, and regulating the quantity of liquid or vgas admitted to the still orA retort; fourth, a uniform and predetermined pressure can be readily secured at the bottom ofthe still, by regulating the height or column of the I bath, and, fifth regardless of the pressure at the lbottom of the still, the pressure at the top, above the molten metal, maybe varied as desired, e., at, above, or below, atmospheric pressure. Advantages lof the process, other than those enumerated, will appear from the hereinafter description.

As examples of the liquids which may be be operated upon, though not the exclusive ones, may be mentioned petroleumand its distillates, either individually or collectively, and oils obtained from the distillation of coal, shale, peat, lignite, and similar materials. ther liquids which may be treated will readily suggest themselves to those skilled in the art, such, e. g., as turpentine, tar, asphalt, etc. I

Among the numerous gases which may be treated may be mentioned coal gas, oil gas, natural gas, and gases obtained from the distillation of wood, lignite, and similar materials.

Among the solids which may be operated upon may be mentioned paraffin and other waxes, asphalt, resin. and various other solids-which 4may be dissolved or otherwlse liquefied. Paraflins may be readily con` verted into olelins through the employment of the present invention.

Features of the process, and their advantages, other than those referred to, will be apparent from the hereinafter detailed description taken in conjunction with the accompanying drawings. q

' In the accompanying drawings, one form` of apparatus is shown which may be success-A fully employed in practising the several processes, but said yapparatus is merely u typical, and the processes, as will be obvious 'tofthose skilled in the art, may be carried out in other forms lof apparatus.-

Referring to the jdrawings, Figure 1 shows, partly in section and partly in ele- 19 vation, a complete apparatusfor the treatment of gases, liquids or s`ol1ds. Fig. 2 is a sectional view of a still which may', be advantageously employed inv the manufacture oflampblack, and I '-lig. 3, shows a simple type of still or retortffor distilling purposes.

In'` the drawings, A

1s a retort or still,

` B l'a liquid separator connected with the out-I let-therefrom, C a pressure or vacuum pump i 20 nlthe system, D a condenser, and E a receivingchamber for the condensates, wherein-the non-condensible ases. are separated.

.StillgA contains a mo ten metal or bath,

preferably of lead, a, and it is manifest that the column of molten metal may be of any desiredl height therebyl providing means for controllin the pressure within the still, particular y at the bottom thereof.

i fA main b is provided for introducing oil orother liquid into the still through rbranch ipe b', controlled by valve b2.- Main b may iieprovided with a preheater b3, which, as

shown, is in the form of a coil which may be heated by a gas'burner b4, which receives -Sti its supply from a branch pipe b5 leading from a gas main G, said branch pipe b5 being provlded with a regulating Ivalve be.

It will be noted that branch ipe -b' extends l within the molten metal. am b is also .4 .provided with another valve controlled branch b", having a discharge outlet bs located above the surface o' the molten metal, whereby oil or other liquid may be delivered onl top of the molten metal, in- 'steadof within the body of the metal.

Another feed main 'o is provided for in-A troducing gas into the still or retort, beneath the surface of the molten metal, said plpe c being provided with a pre-heater 5 c', heated by a burner c* which receives its -supply of gas from a valve-controlled pipe of. The downtake c from branch c is provided with a valve c7, said downtake pipe having its outlet ce located below the sur`- face of'the molten metal.

Still or retort A may be heated in any desired manner, but I have shown a gasheater H, which received its supply from gas mam G, said main being provided with 60 a'manually operated valve h and athermostatically controlled valve h. A well known t pe of thermostat is illustrated for control- -lm the supply of gas to the burner H, em-

an expansible member ,h2 within ,bo ym the sti which, when the temperature1 of u the qua-ntit still througli .shown similar parts 82 and .93.

shutting off, the supply o gas until the temperature is reduced to the desired point, whereupon expansible member h2, by its contraction, causes a break in the electr1c circuit, .with the result that valve h reopens automatically. Similar thermostatic controlling devices may b e employed to regulate,

of material admitted tothe have shown, agramatically, a valve s and thermostatic control s. In pipe b I have As the temperature of the still rises above a predetermined poirit, valve s orv s2 automatically opens and admits a larger quantity of material to the still.

-Still A may be lprovided with thegcustomary regulating devices, suc-h as a pyrometer d, anda pressure or vacuum gage d', and eedmains b and c lmay also be dpipes o and b. In pipe c, I:

provided with, pressure or vacuum vgages l2 and d3, respectively. If the materials introduced through the pipes b and c are to be introduced below the surface of thel molten bath, they will naturally be under pressure and the gages d2 and d3 will then be pressure ages, but if such materials are to be intro uced above the surface of the molten metal, these gages may be vacuum gages- Main c has a downtake e, provided with a valve e', the outlet e2 being positioned above the surface of the molten metal in the still. This pipe may be employed for blowing out of the still the lampblack or other similar products which may separate at the surface of the molten metal, orI

may be used to carry away the vapors which accumulate at the top of the still.

The temperature at the top of the still may be controlled by water or other refrigerating liquid entering through main g, through valve g', and nozzle g2, by which it' is sprayed on the top of the still, and flows 1nto trough g3, whence it is drawn oi through waste-pipe g4. n

The separator or trap B is of any well known type, and the liquid or liquids which accumulate therein may be drawnl off through valve z'. Separator B has a direct connection with vacuum or pressure pump C, through a hand-controlled valve 2 and the flap valve 3, the flap in this valve being so arranged as to permit the gases to iow to' pump C, but precluding their return. The outlet from pump C is connected to the inlet of coil D of condenser D, a ap valve z" precluding the return of gases to the pump, and a pressure or vacuum gage d* indicating the pressure, plus or minus, at

weaves which the gases enter the condensing coil. A by-pass C', having controlling valves j j", may. be introduced inthe system, whereby the gases from separator B may be passed direfctly into the condensing coil D, z'.

p without passing them through pump C.

A stood that coil liquids accumulate,

Condenser D is -provided with an inlet and an outlet k k', reslpectively,for the refrigerating medium a though it will be under'- D may be cooled in other ways, as e. l,1.,.by an expanding gas. xThe outlet of co1] D leads to the separator or receiving chamber E, wherein the condensed from which they lmay be withdrawn through valve j. Thefgases which are not condensed pass from the top of separator E into pipe l, which isproulating the valve Z2.

II is provided with a valfe o,

vided with a pressure or vacuum gage Z',- anda manually controlled valve Z2. It will be understood that the pressure on the system 1'may be controlled, as desired, bys reg- In other words, by controlling the flow of the residual gases through said valve, a back pressure may be produced upon the system.

Referring to the apparatus shown in Fig.- 2, which is especially adapted for making lampblack, A is the still or retort containing the molten lead or other metal w', heated by gas-burner H or other suitable heating means. It has a liquid or gaseous inlet m, dipping below the surface of bath a-, in which may be located apre-heater m', hand valve m2, and pressure or vacuum gage m3. It may also, if desired, be provided with a stirrer, J, operated from a Apulley K, for keepin the molten metal agitated. l Its outlet n eads to ya receptacle or chamber I, wherein lampblack is deposited. Chamber normally open, but which may be closed to permit the removal of the lampblack whichaccumulates in. the bottom 4of the. chamber without interfering with the operation of the apparatus. At the top of chamber I is an inclined baiie p, which delects the separated lamp-` black, and an outlet pipe g for the escape of residual gases. Retort A is provided with a ga's inlet pipe g', for blowing the separated lampblack out of the retort Ainto Ichamber I. Pipe g may, if desired,

eter.

'm (Fig. e),

tort is provided with a suitable inlet r and outlet r. Still A2 may also be provided with some of the accessories, previously/ described in connection with still A, such as a thermostat, pre-heater, gages, and pyrom- The upper part ofthe still A2 may, moreover, be coiled in the manner shown with reference 'to the still A. Having fully described f the apparatus, and its general mode of operation, as well as a. number of the materials which maybe treated, brief reference will be made to a few of the specific processes which may be practised. r

Assuming 'a liquid, e. g., or any of its'fractions, may be introduced into still b and branch b" onto thel surface of the molten metal. This operation may be similarly carried out in retort A2, Fig. 3. By manipulating the apparatus, as described, and desiredv pressure, from plus. to minus, may be produced in the top of the still. The various products of distillation may be separated, as described, it being understood that a plurality of separators B, condensers D and traps E may be used if desired, only single ones .ha-ving been shown to avoid undue complication ofthe drawing.

If it be desired to crack or polymerize a liquid (or dissolved solid), it may be introduced through main b and branch b beneath the surface of the molten lead. The result ing products pass off and may be collected or separated as described.

In making lampblack, e. g., the liquid crude petroleum,

A through main hydrocarbon or gas may be introduced beneath the surface of the lead through pipe and the separated carbon blown into chamber I, by a suitable blast of gaseons, fluid, pre-heated if desired, introduced through pipe q (Fig. 2) or branch pipe'e.

of main C (Fig. 1). In this and similar processes, the top of the still or retort may be advantageously cooled by water or`other refrigerant suppliedI by rose g2, Fig. 1.

The foregoing processes are merely illustrative, since the broad invention resides inthe manner in which the temperature and pressure of various chemical operations may be accurately controlled, and different pressures and temperatures obtained in the bottom and top, respectively, of the still or retort. Accordingly, various processes, other than those described, as well as modifications and variations thereof, to meet the exigencies of any particular process, will readilysuggest themselves to those skilled in the art. That is to say, the processes outlined are typical and suggestive, only, and do not preclude the application of the broad principles disclosedto volving analogous operations.

When the still is not in use, the molten lead may be drawn oil' through pipe L into processes inany , heated). The receptacle may then-sbc eledpur whatI claimjas new, and desire to secure c vated, and, when it `is desired to further use theI still, the lead may be remelted, and allowed to flow into the still by gravity.`

i. -Any suitable combinations of metals or alloys.l

ses, in lieu of the lead bath. f aving thusfully described the invention,

by Letters Patent, is: g il 1. Increasing the illuminating value of natural gas by converting the paraiiins' into olefns by bringing said as into contact with a molten bath of meta 12. The process of distilling hydrocarbons, which consists in.. bringing 'them in contact with molten metal, producing a partial vacuum by exhaustion at the ,upper part of the still and cooling the upperpart of the'still externally.

3.' The process of /altering the composi-V tion' of petroleum distillates'which consists` in introducing the distillates under pressure into a metal bath Vcontained in a still near the bottom of said bath, and maintaining the upper portion of the still above the surface of the bath under a partial vacuum. 4.- The recess of increasingthe condensable constituents of a hydrocarbon as which consists lin passing the gas throu li molten metal and cracking said gas by t e heat of such molten metal. y

5: The process of treating hydrocarbons which -consists in introducing them on to thelsurface of molten metal and comming'ling, with the resulting va ors, gases passed through the molten meta 6.l The process of distillin hydrocarbons which consists in bringingt em in contact may'be used in the still, for specific vwith `molten metal, and pxroducing a partial vacuum by exhausting t e upper partof a s till contained inthe molten'metal.

7. The process of altering the composition of petroleumdistillates which consists in passing them throu h molten metal --contained ina still Aan producing a partial vacuum by exhaustion'at the upper part of the still. A'

s 8. The process of altering the composition of petroleum distillates which consists, in passing them throu h molten metal` and'under' pressure contro led by 'the height of the molten metal.

1 9. The process of altering the-compositiony of petroleum distillates' which consists in lntroducing them into a` bath of molten fmetallb'elow the surface ofy said metal ap- 'plying suicient pressure to the distillates during the introduction to overcome the hydrostatic pressure of the molten bath and malntaining a partial 'vacuum in the still above the bath by exhaustion. v

10. The process of altering the composition of petroleum distillates which consists in passing them throughV molte'ii` metal and thereafter compressing and condensing the products of the cracking operation.

11. The ,process of altering the composition of petroleum distillates which consists in .introducing the'distillates below the surface of amolten metal bath under suicient pressure toovercome the hydrostatic pressure of the molten metal, maintaining a partial vacuum above the' surface of the molten metal bath and condensing the products of the cracking operation.

In testimony whereof I have signed my name to this s eciication..

AIIGUSTE J. PARIS, Jn. 

